Full text of DOI:10.1016/S0022-1139(00)81705-4

178
on the reaction and on the purity of
one preparation was under-
(270 Torr) and
(400 Torr). The only detectable impurity was a very small amount of
taken using the maximum pressure attainable of
(0.2%). Hence it must be concluded that
manner could also be contaminated by traces of
prepared in this
(0.4%).
Since the formation of
it appears advisable to work with large excess of
extent of contamination by
depends on the relative amounts of
In this way the
can be reduced still further.
and
Preparation of
In this case the reaction conditions were controlled very carefully. The
temperature of the water circulating through the glass finger was maintained
between 20
kept below 30
of SO, (0.02 mol), 20
and 25
by the use of a forced air stream. After evacuation, 50 Torr
of and 700 Torr of OF, were introduced into
and when necessary the reactor temperature was
the reactor. The mixture was irradiated for 57 min when it was calculated that
80% of the SO, had reacted on the basis of an average change of pressure
with time of 0.7 Torr
-130 (removing SO, +
and some 0,). A residual pressure of
The mixture was fractionally condensed at
and at -196 (removing
10 Torr in the reactor had no effect
+
on the preparation of a second batch of products. In this case after a new
portion of SO, had been introduced into the reactor, the mixture of
and
removed from the first batch at -196
was recycled, being allowed to
evaporate into the reactor under controlled conditions.
The product was again purified by trap-to-trap distillation. A small
amount of substance obtained as a head fraction at -115
and the volatile residue remaining at -95 (pure
The vapor pressure equation previously reported
incorrect. The correct equation which is for temperatures between
-75 and -25 is logp(Torr) 7.851 1340/T. The extrapolated boil-
ing point is -3.5 and the constant is 22.7.
was discarded
was retained.
for
is
*Caution:
be handled very carefully. In the course of our studies we have-had two
explosions: One was caused by reaction of with organic matter and
was suddenly warmed up to
is a strong oxidizing agent and the compound should
the other when solid
- 2 0
at -196